HRID1025480

反应详情

EQUATION

反应方程式

HRID 1025480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of 4-chloro-7,8-dimethyl-imidazo[1,2-a]quinoxaline (32.2 g, 0.148 mot) in THF/NMP 2:1 (312 mL) was added NBS (26.3 g, 0.148 mot) in one portion at room temperature. After stirred for 18 h, additional NBS (13.1 g, 0.074 mot) was added and the mixture was stirred for additional 2 h at room temperature. After removal of the THF portion of the organic phase by vacuum evaporation, water was added (520 mL). The precipitate was filtered and the residue was washed with water, diethyl ether and dried to give 35 g of the title compound. 1H-NMR (300 MHz, d6-DMSO): δ=8.54 (1H, s), 7.75 (1H, s), 7.40 (1H, s), 2.20 (6H, s) ppm.

WORKUP

后处理

  1. stirringthe mixture was stirred for additional 2 h at room temperature
  2. customAfter removal of the THF portion of the organic phase
  3. customby vacuum evaporation, water
  4. additionwas added (520 mL)
  5. filtrationThe precipitate was filtered
  6. washthe residue was washed with water, diethyl ether
  7. customdried